CN110591286A - Graphene-based polymer composite material and preparation process thereof - Google Patents
Graphene-based polymer composite material and preparation process thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
Abstract
The invention discloses a medicine, which comprises the following components: graphite, strong protonic acid, ascorbic acid, potassium permanganate, ethanol, isocyanic acid, polystyrene, N-dimethylformamide, epoxy resin and an initiator, wherein the mass percentages of the components are as follows: 20-30% of graphite, 15-25% of strong protonic acid, 10-20% of ascorbic acid, 2-4% of potassium permanganate, 15-25% of ethanol, 10-20% of isocyanic acid, 1-3% of polystyrene, 0.5-1% of N, N-dimethylformamide, 5-10% of epoxy resin and 0.5-1% of initiator, wherein the preparation process comprises the following steps of selecting raw materials; step two, preparing graphene; step three, irradiation reduction; step four, compounding the polymer; step five, washing and processing; and step six, quality inspection and packaging, wherein the specific surface area of the polymer composite material of the graphene is greatly increased, so that the density of the polymer composite material of the graphene is higher, and the service life of the polymer composite material of the graphene is prolonged.
Description
Technical Field
The invention relates to the technical field of graphene materials, in particular to a graphene-based polymer composite material and a preparation process thereof.
Background
Graphene is a two-dimensional carbon nanomaterial which is formed by sp hybridized orbitals to form a hexagonal honeycomb lattice, has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, is considered to be a revolutionary material in the future, and is generally processed into a polymer composite material for use; the traditional graphene polymer composite material has high cost and high manufacturing cost, is not beneficial to processing and production, and meanwhile, the specific surface area of the traditional graphene polymer composite material cannot be increased during processing, so that the density is low, the tensile resistance is low, the composite material is extremely easy to break, and is not beneficial to users to use; in view of these drawbacks, it is necessary to design a graphene-based polymer composite and a preparation process thereof.
Disclosure of Invention
The invention aims to provide a graphene-based polymer composite material and a preparation process thereof, so as to solve the problems in the background art.
In order to solve the technical problems, the invention provides the following technical scheme: a graphene-based polymer composite, the formulation comprising: graphite, strong protonic acid, ascorbic acid, potassium permanganate, ethanol, isocyanic acid, polystyrene, N-dimethylformamide, epoxy resin and an initiator, wherein the mass percentages of the components are as follows: 20-30% of graphite, 15-25% of strong protonic acid, 10-20% of ascorbic acid, 2-4% of potassium permanganate, 15-25% of ethanol, 10-20% of isocyanic acid, 1-3% of polystyrene, 0.5-1% of N, N-dimethylformamide, 5-10% of epoxy resin and 0.5-1% of initiator.
A preparation process of a graphene-based polymer composite material comprises the following steps of firstly, selecting raw materials; step two, preparing graphene; step three, irradiation reduction; step four, compounding the polymer; step five, washing and processing; step six, quality inspection and packaging;
in the first step, the components in percentage by mass are as follows: selecting 20-30% of graphite, 15-25% of strong protonic acid, 10-20% of ascorbic acid, 2-4% of potassium permanganate, 15-25% of ethanol, 10-20% of isocyanic acid, 1-3% of polystyrene, 0.5-1% of N, N-dimethylformamide, 5-10% of epoxy resin and 0.5-1% of initiator, and weighing according to the sum of the weight percentages of 1;
in the second step, the preparation of the graphene comprises the following steps:
1) manually cleaning the reaction kettle, adding graphite, and keeping the temperature at normal temperature;
2) putting potassium permanganate into a reaction kettle, adding a certain amount of strong protonic acid, and stirring while adding the strong protonic acid;
3) stopping stirring, sealing the reaction kettle, and reacting for 1-2h to obtain graphite oxide;
4) placing the obtained graphite oxide in a ceramic crucible, placing the ceramic crucible in a muffle furnace, heating for 30s, and taking out;
5) putting the heated graphite oxide into an aqueous solution, and putting the graphite oxide into an ultrasonic machine for ultrasonic stripping for 20min to obtain a graphene suspension;
6) putting the obtained graphene suspension into a refrigerator for freeze drying to obtain graphene;
in the third step, the graphene obtained in the second step is stored by using a ceramic barrel, ascorbic acid is added, the graphene is uniformly stirred and then placed in an irradiation machine, and ultraviolet rays are used for irradiating for 1-2 hours;
in the fourth step, the polymer compounding comprises the following steps:
1) manually putting graphene into a reaction kettle, adding isocyanic acid, and keeping the temperature at normal temperature;
2) sequentially putting polystyrene and N, N-dimethylformamide into a reaction kettle, and uniformly stirring;
3) stopping stirring, sealing the reaction kettle, and filling inert gas for reaction for 1-2 h;
4) opening the reaction kettle, adding epoxy resin and an initiator, uniformly stirring, and continuously reacting for 30min to obtain a graphene polymer solution;
in the fifth step, the graphene polymer solution obtained in the fourth step is cooled, added with ethanol and washed with water to obtain a graphene polymer material;
and in the sixth step, the graphene polymer material obtained in the fifth step is manually inspected, and is packed in a box after being inspected to be qualified, and is stored in a shade.
According to the technical scheme, the components are as follows by mass percent: 20% graphite, 16% strong protonic acid, 20% ascorbic acid, 4% potassium permanganate, 15% ethanol, 15% isocyanic acid, 3% polystyrene, 1% N, N-dimethylformamide, 5% epoxy resin and 1% initiator.
According to the technical scheme, the strong protonic acid is concentrated sulfuric acid, fuming nitric acid or a mixture of the concentrated sulfuric acid and the fuming nitric acid.
According to the technical scheme, the initiator is a free radical polymerization initiator.
According to the technical scheme, the internal temperature of the muffle furnace used in the second step 4) is 1050 ℃.
According to the technical scheme, products which are not qualified in the step six are subjected to re-melting and reworking.
Compared with the prior art, the invention has the following beneficial effects: the method has the advantages that the method is safe and reliable, the specific surface area of the polymer composite material of the graphene is greatly increased, the density of the polymer composite material of the graphene is higher, the tensile strength of the polymer composite material of the graphene is increased, the service life of the polymer composite material of the graphene is prolonged, the resistivity and the heat conductivity coefficient of the polymer composite material of the graphene are greatly increased, the use by a user is facilitated, the method is simple and precise in process, the other expensive polymer composite material of the graphene can be replaced, the effect is obvious, the raw materials are cheap and low in cost, the processing is convenient, the production cost is greatly saved, and the processing and the production are facilitated.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution: a graphene-based polymer composite material and a preparation process thereof are disclosed:
example 1:
a graphene-based polymer composite, the formulation comprising: graphite, strong protonic acid, ascorbic acid, potassium permanganate, ethanol, isocyanic acid, polystyrene, N-dimethylformamide, epoxy resin and an initiator, wherein the mass percentages of the components are as follows: 20% graphite, 16% strong protonic acid, 25% ascorbic acid, 4% potassium permanganate, 15% ethanol, 10% isocyanic acid, 3% polystyrene, 1% N, N-dimethylformamide, 5% epoxy resin and 1% initiator.
A preparation process of a graphene-based polymer composite material comprises the following steps of firstly, selecting raw materials; step two, preparing graphene; step three, irradiation reduction; step four, compounding the polymer; step five, washing and processing; step six, quality inspection and packaging;
in the first step, the components in percentage by mass are as follows: selecting 20-30% of graphite, 15-25% of strong protonic acid, 10-20% of ascorbic acid, 2-4% of potassium permanganate, 15-25% of ethanol, 10-20% of isocyanic acid, 1-3% of polystyrene, 0.5-1% of N, N-dimethylformamide, 5-10% of epoxy resin and 0.5-1% of initiator, and weighing according to the sum of the weight percentages of 1;
in the second step, the preparation of the graphene comprises the following steps:
1) manually cleaning the reaction kettle, adding graphite, and keeping the temperature at normal temperature;
2) putting potassium permanganate into a reaction kettle, adding a certain amount of strong protonic acid while stirring, wherein the strong protonic acid is concentrated sulfuric acid, fuming nitric acid or a mixture of the concentrated sulfuric acid and the fuming nitric acid;
3) stopping stirring, sealing the reaction kettle, and reacting for 1-2h to obtain graphite oxide;
4) placing the obtained graphite oxide in a ceramic crucible, placing the ceramic crucible in a muffle furnace, heating for 30s, and taking out, wherein the internal temperature of the muffle furnace is 1050 ℃;
5) putting the heated graphite oxide into an aqueous solution, and putting the graphite oxide into an ultrasonic machine for ultrasonic stripping for 20min to obtain a graphene suspension;
6) putting the obtained graphene suspension into a refrigerator for freeze drying to obtain graphene;
in the third step, the graphene obtained in the second step is stored by using a ceramic barrel, ascorbic acid is added, the graphene is uniformly stirred and then placed in an irradiation machine, and ultraviolet rays are used for irradiating for 1-2 hours;
in the fourth step, the polymer compounding comprises the following steps:
1) manually putting graphene into a reaction kettle, adding isocyanic acid, and keeping the temperature at normal temperature;
2) sequentially putting polystyrene and N, N-dimethylformamide into a reaction kettle, and uniformly stirring;
3) stopping stirring, sealing the reaction kettle, and filling inert gas for reaction for 1-2 h;
4) opening the reaction kettle, adding epoxy resin and an initiator, uniformly stirring, and continuously reacting for 30min to obtain a graphene polymer solution, wherein the initiator is a free radical polymerization initiator;
in the fifth step, the graphene polymer solution obtained in the fourth step is cooled, added with ethanol and washed with water to obtain a graphene polymer material;
and in the sixth step, the graphene polymer material obtained in the fifth step is manually inspected, the graphene polymer material is boxed and packaged after being inspected to be qualified, the packaged graphene polymer material is stored in a shade, and products which are not qualified in inspection are re-melted and reworked.
Example 2:
a graphene-based polymer composite, the formulation comprising: graphite, strong protonic acid, ascorbic acid, potassium permanganate, ethanol, isocyanic acid, polystyrene, N-dimethylformamide, epoxy resin and an initiator, wherein the mass percentages of the components are as follows: 20% graphite, 16% strong protonic acid, 20% ascorbic acid, 4% potassium permanganate, 15% ethanol, 15% isocyanic acid, 3% polystyrene, 1% N, N-dimethylformamide, 5% epoxy resin and 1% initiator.
A preparation process of a graphene-based polymer composite material comprises the following steps of firstly, selecting raw materials; step two, preparing graphene; step three, irradiation reduction; step four, compounding the polymer; step five, washing and processing; step six, quality inspection and packaging;
in the first step, the components in percentage by mass are as follows: selecting 20-30% of graphite, 15-25% of strong protonic acid, 10-20% of ascorbic acid, 2-4% of potassium permanganate, 15-25% of ethanol, 10-20% of isocyanic acid, 1-3% of polystyrene, 0.5-1% of N, N-dimethylformamide, 5-10% of epoxy resin and 0.5-1% of initiator, and weighing according to the sum of the weight percentages of 1;
in the second step, the preparation of the graphene comprises the following steps:
1) manually cleaning the reaction kettle, adding graphite, and keeping the temperature at normal temperature;
2) putting potassium permanganate into a reaction kettle, adding a certain amount of strong protonic acid while stirring, wherein the strong protonic acid is concentrated sulfuric acid, fuming nitric acid or a mixture of the concentrated sulfuric acid and the fuming nitric acid;
3) stopping stirring, sealing the reaction kettle, and reacting for 1-2h to obtain graphite oxide;
4) placing the obtained graphite oxide in a ceramic crucible, placing the ceramic crucible in a muffle furnace, heating for 30s, and taking out, wherein the internal temperature of the muffle furnace is 1050 ℃;
5) putting the heated graphite oxide into an aqueous solution, and putting the graphite oxide into an ultrasonic machine for ultrasonic stripping for 20min to obtain a graphene suspension;
6) putting the obtained graphene suspension into a refrigerator for freeze drying to obtain graphene;
in the third step, the graphene obtained in the second step is stored by using a ceramic barrel, ascorbic acid is added, the graphene is uniformly stirred and then placed in an irradiation machine, and ultraviolet rays are used for irradiating for 1-2 hours;
in the fourth step, the polymer compounding comprises the following steps:
1) manually putting graphene into a reaction kettle, adding isocyanic acid, and keeping the temperature at normal temperature;
2) sequentially putting polystyrene and N, N-dimethylformamide into a reaction kettle, and uniformly stirring;
3) stopping stirring, sealing the reaction kettle, and filling inert gas for reaction for 1-2 h;
4) opening the reaction kettle, adding epoxy resin and an initiator, uniformly stirring, and continuously reacting for 30min to obtain a graphene polymer solution, wherein the initiator is a free radical polymerization initiator;
in the fifth step, the graphene polymer solution obtained in the fourth step is cooled, added with ethanol and washed with water to obtain a graphene polymer material;
and in the sixth step, the graphene polymer material obtained in the fifth step is manually inspected, the graphene polymer material is boxed and packaged after being inspected to be qualified, the packaged graphene polymer material is stored in a shade, and products which are not qualified in inspection are re-melted and reworked.
Example 3:
a graphene-based polymer composite, the formulation comprising: graphite, strong protonic acid, ascorbic acid, potassium permanganate, ethanol, isocyanic acid, polystyrene, N-dimethylformamide, epoxy resin and an initiator, wherein the mass percentages of the components are as follows: 20% graphite, 16% strong protonic acid, 15% ascorbic acid, 4% potassium permanganate, 15% ethanol, 20% isocyanic acid, 3% polystyrene, 1% N, N-dimethylformamide, 5% epoxy resin and 1% initiator.
A preparation process of a graphene-based polymer composite material comprises the following steps of firstly, selecting raw materials; step two, preparing graphene; step three, irradiation reduction; step four, compounding the polymer; step five, washing and processing; step six, quality inspection and packaging;
in the first step, the components in percentage by mass are as follows: selecting 20-30% of graphite, 15-25% of strong protonic acid, 10-20% of ascorbic acid, 2-4% of potassium permanganate, 15-25% of ethanol, 10-20% of isocyanic acid, 1-3% of polystyrene, 0.5-1% of N, N-dimethylformamide, 5-10% of epoxy resin and 0.5-1% of initiator, and weighing according to the sum of the weight percentages of 1;
in the second step, the preparation of the graphene comprises the following steps:
1) manually cleaning the reaction kettle, adding graphite, and keeping the temperature at normal temperature;
2) putting potassium permanganate into a reaction kettle, adding a certain amount of strong protonic acid while stirring, wherein the strong protonic acid is concentrated sulfuric acid, fuming nitric acid or a mixture of the concentrated sulfuric acid and the fuming nitric acid;
3) stopping stirring, sealing the reaction kettle, and reacting for 1-2h to obtain graphite oxide;
4) placing the obtained graphite oxide in a ceramic crucible, placing the ceramic crucible in a muffle furnace, heating for 30s, and taking out, wherein the internal temperature of the muffle furnace is 1050 ℃;
5) putting the heated graphite oxide into an aqueous solution, and putting the graphite oxide into an ultrasonic machine for ultrasonic stripping for 20min to obtain a graphene suspension;
6) putting the obtained graphene suspension into a refrigerator for freeze drying to obtain graphene;
in the third step, the graphene obtained in the second step is stored by using a ceramic barrel, ascorbic acid is added, the graphene is uniformly stirred and then placed in an irradiation machine, and ultraviolet rays are used for irradiating for 1-2 hours;
in the fourth step, the polymer compounding comprises the following steps:
1) manually putting graphene into a reaction kettle, adding isocyanic acid, and keeping the temperature at normal temperature;
2) sequentially putting polystyrene and N, N-dimethylformamide into a reaction kettle, and uniformly stirring;
3) stopping stirring, sealing the reaction kettle, and filling inert gas for reaction for 1-2 h;
4) opening the reaction kettle, adding epoxy resin and an initiator, uniformly stirring, and continuously reacting for 30min to obtain a graphene polymer solution, wherein the initiator is a free radical polymerization initiator;
in the fifth step, the graphene polymer solution obtained in the fourth step is cooled, added with ethanol and washed with water to obtain a graphene polymer material;
and in the sixth step, the graphene polymer material obtained in the fifth step is manually inspected, the graphene polymer material is boxed and packaged after being inspected to be qualified, the packaged graphene polymer material is stored in a shade, and products which are not qualified in inspection are re-melted and reworked.
The properties of the examples are compared in the following table:
| tensile strength/MPa | Specific surface area/m2/g | Resistivity/p | Thermal conductivity/W/m-k | |
| Example 1 | 42 | 310 | 1.2*10-6 | 5200 |
| Example 2 | 40 | 336 | 0.8*10-6 | 5400 |
| Example 3 | 43 | 302 | 1.0*10-6 | 5300 |
Based on the above, the invention has the advantages that the invention is safe and reliable, the graphene is obtained by oxidation reduction, muffle furnace heating and ultrasonic stripping by using graphite as a raw material, the polymer composite material of the graphene is obtained by irradiation and polymerization reaction of an irradiation machine, the specific surface area of the polymer composite material of the graphene is greatly improved, the density of the polymer composite material of the graphene is higher, the tensile strength of the polymer composite material of the graphene is improved, the service life of the polymer composite material of the graphene is prolonged, the resistivity and the heat conductivity coefficient of the polymer composite material of the graphene are greatly improved, the use by a user is facilitated, the process is simple and precise, other expensive polymer composite materials of the graphene can be replaced, the effect is obvious, the raw material is cheap and has low cost, the processing is convenient, and the production cost is greatly saved, is beneficial to processing and production.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A graphene-based polymer composite, the formulation comprising: graphite, strong protonic acid, ascorbic acid, potassium permanganate, ethanol, isocyanic acid, polystyrene, N-dimethylformamide, epoxy resin and an initiator, and is characterized in that: the weight percentage of each component is as follows: 20-30% of graphite, 15-25% of strong protonic acid, 10-20% of ascorbic acid, 2-4% of potassium permanganate, 15-25% of ethanol, 10-20% of isocyanic acid, 1-3% of polystyrene, 0.5-1% of N, N-dimethylformamide, 5-10% of epoxy resin and 0.5-1% of initiator.
2. A preparation process of a graphene-based polymer composite material comprises the following steps of firstly, selecting raw materials; step two, preparing graphene; step three, irradiation reduction; step four, compounding the polymer; step five, washing and processing; step six, quality inspection and packaging; the method is characterized in that:
in the first step, the components in percentage by mass are as follows: selecting 20-30% of graphite, 15-25% of strong protonic acid, 10-20% of ascorbic acid, 2-4% of potassium permanganate, 15-25% of ethanol, 10-20% of isocyanic acid, 1-3% of polystyrene, 0.5-1% of N, N-dimethylformamide, 5-10% of epoxy resin and 0.5-1% of initiator, and weighing according to the sum of the weight percentages of 1;
in the second step, the preparation of the graphene comprises the following steps:
1) manually cleaning the reaction kettle, adding graphite, and keeping the temperature at normal temperature;
2) putting potassium permanganate into a reaction kettle, adding a certain amount of strong protonic acid, and stirring while adding the strong protonic acid;
3) stopping stirring, sealing the reaction kettle, and reacting for 1-2h to obtain graphite oxide;
4) placing the obtained graphite oxide in a ceramic crucible, placing the ceramic crucible in a muffle furnace, heating for 30s, and taking out;
5) putting the heated graphite oxide into an aqueous solution, and putting the graphite oxide into an ultrasonic machine for ultrasonic stripping for 20min to obtain a graphene suspension;
6) putting the obtained graphene suspension into a refrigerator for freeze drying to obtain graphene;
in the third step, the graphene obtained in the second step is stored by using a ceramic barrel, ascorbic acid is added, the graphene is uniformly stirred and then placed in an irradiation machine, and ultraviolet rays are used for irradiating for 1-2 hours;
in the fourth step, the polymer compounding comprises the following steps:
1) manually putting graphene into a reaction kettle, adding isocyanic acid, and keeping the temperature at normal temperature;
2) sequentially putting polystyrene and N, N-dimethylformamide into a reaction kettle, and uniformly stirring;
3) stopping stirring, sealing the reaction kettle, and filling inert gas for reaction for 1-2 h;
4) opening the reaction kettle, adding epoxy resin and an initiator, uniformly stirring, and continuously reacting for 30min to obtain a graphene polymer solution;
in the fifth step, the graphene polymer solution obtained in the fourth step is cooled, added with ethanol and washed with water to obtain a graphene polymer material;
and in the sixth step, the graphene polymer material obtained in the fifth step is manually inspected, and is packed in a box after being inspected to be qualified, and is stored in a shade.
3. The graphene-based polymer composite according to claim 1, wherein: the components are as follows by mass percent: 20% graphite, 16% strong protonic acid, 20% ascorbic acid, 4% potassium permanganate, 15% ethanol, 15% isocyanic acid, 3% polystyrene, 1% N, N-dimethylformamide, 5% epoxy resin and 1% initiator.
4. The graphene-based polymer composite according to claim 1, wherein: the strong protonic acid is concentrated sulfuric acid, fuming nitric acid or a mixture thereof.
5. The graphene-based polymer composite according to claim 1, wherein: the initiator is a free radical polymerization initiator.
6. The process for preparing a graphene-based polymer composite according to claim 2, wherein: the muffle furnace used in the second step 4) has an internal temperature of 1050 ℃.
7. The process for preparing a graphene-based polymer composite according to claim 2, wherein: and in the sixth step, products which are detected to be unqualified are subjected to furnace returning and reworking.
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Application publication date: 20191220 |
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